CN106185906A - A kind of Graphene elastic film and preparation method thereof - Google Patents
A kind of Graphene elastic film and preparation method thereof Download PDFInfo
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- CN106185906A CN106185906A CN201610566947.8A CN201610566947A CN106185906A CN 106185906 A CN106185906 A CN 106185906A CN 201610566947 A CN201610566947 A CN 201610566947A CN 106185906 A CN106185906 A CN 106185906A
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- C01B2204/00—Structure or properties of graphene
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
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- C01B2204/26—Mechanical properties
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a kind of Graphene elastic film and preparation method thereof, this graphene film is obtained through solution film forming and chemical reduction step by graphene oxide.This graphene film is consisted of physical crosslinking macroscopical multilayered fold Graphene with micro-scale fold；In vertical direction, thin film has double-decker, and interlayer is linked by multi-layer graphene film；In horizontal direction, thin film is made up of elastic through hemispherical fluctuating, and ball wall has fold, therefore has high vertical compression elasticity and horizontal stretch is elastic.This thin film has fabulous flexibility, and doubling does not leave folding line more than 100,000 times repeatedly.This high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and elastic failure percentage elongation is 30 50%, and compression ratio is 80 90%, and conductivity is 600 1000S/cm, can be used as high-elastic conductive devices.
Description
Technical field
The present invention relates to novel elastic graphene film material and preparation method thereof, particularly relate to a kind of Graphene elastic film
And preparation method thereof.
Background technology
2010, two of Univ Manchester UK professor Andre GeiM and Konstantin Novoselov because
It is successfully separated out stable Graphene first and obtains Nobel Prize in physics, start the upsurge that Graphene is studied by the whole world.
Graphene has excellent electric property, and (under room temperature, electron mobility is up to 2 × 105cM2/ Vs), prominent heat conductivility (5000W/
(MK), extraordinary specific surface area (2630M2/ g), its Young's modulus (1100GPa) and fracture strength (125GPa).Graphene is excellent
Different electrical and thermal conductivity performance is well beyond metal, and Graphene has an advantage of corrosion-and high-temp-resistant simultaneously, and its good machinery
Performance and relatively low density more allow it possess the potentiality at thermo electric material field substituted metal.
Macroscopic view assembles the important application form that graphene oxide membrane is nanoscale graphite alkene, and conventional preparation method is
Suction method, scrape embrane method, spin-coating method, spraying process and dip coating etc..
But, the most prepared graphene film does not have high stretching high resiliency, it is impossible to obtain in terms of high resiliency device
Application.Within 16 years, professor Shi Gaoquan creates a lot of huge folds by the method for macroscopic view template assemblies in graphene membrane surface, does
Arrive the high resiliency stretching of graphene film, but its vertical compression aspect has not related to.Its incomplete elasticity can not meet
The demand of rapid technological growth.And the deficiency of Design of Membrane Structure makes its flexibility be still not clear, and limits it at flexible device
The application of aspect.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of Graphene elastic film and preparation method thereof.
It is an object of the invention to be achieved through the following technical solutions: a kind of Graphene elastic film, described elastic film
Being formed by the crosslinking of two-layer graphene film, described graphene membrane surface has hemispherical protuberances structure, on same layer graphene film
Hemispherical protuberances structure is interconnected；The ball wall of described hemispherical protuberances structure has fold.
Further, the radius 0.1～2mm of described hemispherical protuberances structure, the surface density (unit are of fold on ball wall
The length of upper fold lines) it is 500～2000um/um2
The preparation method of a kind of Graphene elastic film, comprises the steps of:
(1) graphene oxide of 100 weight portions being configured to concentration is 6～30mg/mL graphene oxide water solution, molten
Adding the auxiliary agent of 0.1-10% weight portion (solid content) in liquid, described auxiliary agent is the volatilizable and degradable little molecule of low temperature；
After ultrasonic disperse, it is poured on Die and mould plate, under certain relative air humidity, naturally dries into graphene oxide membrane；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.
(3) graphene film after reduction is placed in the ethanol of 40-90 DEG C 5～10min, to wash away hydroiodic acid, then natural
Dry, obtain Graphene elastic film.
Further, the relative air humidity in described step 1 is 50-80%.
Further, described inorganic salt is in ammonium hydrogen carbonate, ammonium chloride, ammonium carbonate, hydrochloric acid, acetic acid and ammonia
One or more.
Further, described hydroiodic acid Solution H I content is 15 35, and reduction temperature is 70 100 degrees Celsius, reduction
Time is 4-8h.
The beneficial effects of the present invention is: the present invention passes through solution film forming and electronation, give film double-decker, and
Every tunic has the spherical fold of fluctuating to constitute so that it can all have high vertically pressing in vertical and horizontal direction
Contracting is elastic, horizontal stretch is elastic and flexible.Its preparating mechanism is as follows:
Under the effect of the acid of one, little molecule or salt, graphene oxide liquid crystal obtains partial destruction, graphene oxide lamella
Upper negative charge is neutralized so that himself produces a lot of folds.
Two, in high relative humidity film forming procedure, because lacking electrical charge rejection, graphene oxide can not perfect stack,
Fold is retained in graphene oxide membrane.In hydroiodic acid reduction process, on the one hand fold makes hydroiodic acid be easier to
Enter membrane structure so that reduction effect is more preferable；On the other hand, iodine can be made to remain in graphene oxide layer after hydroiodic acid reduction
Between.
Three, during high temperature reduction, volatile salt or acid and I decompose, and constantly produce spilehole,
Make membrane structure thinning, form the 3-D solid structure of many folds.
Its this high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and horizontal resiliency elongation at break is 30-
50%, elastic and vertical compression ratio is 80 90%, and conductivity is 600-1000S/cm, can be used as high-elastic conductive devices.
Accompanying drawing explanation
Fig. 1 is the exterior view of elastic graphite alkene film.
Fig. 2 is the stress strain curve of elastic graphite alkene film.
Fig. 3 is the cross section surface sweeping Electronic Speculum of elastic graphite alkene film.
Fig. 4 is the compression curve of elastic graphite alkene film；
Fig. 5 is the structural representation of elastic film of the present invention, including hemispherical protuberances and pleated structure.
Detailed description of the invention
Below in conjunction with the accompanying drawings and embodiment the invention will be further described.The present embodiment be served only for the present invention is done into
The explanation of one step, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according in foregoing invention
Hold and make some nonessential change and adjustment, belong to protection scope of the present invention.
Embodiment 1:
(1) graphene oxide being configured to concentration is 6mg/mL graphene oxide water solution, adds oxidation stone in the solution
The auxiliary agent of the 0.1% of ink alkene quality, described auxiliary agent is ammonium chloride；After dispersion, it is poured on Die and mould plate at relative air humidity 50%
Lower naturally dry into graphene oxide membrane；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is 15wt%, and reduction temperature is 70 DEG C, and the recovery time is 4h.
(3) graphene film after reduction is placed in 5min in the ethanol of 90 DEG C, to wash away Surface Hydrogen iodic acid, the most naturally dries in the air
Dry, obtain Graphene elastic film.
This high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and horizontal direction elastic failure percentage elongation is
30%, compression ratios is 80%, and conductivity is 600S/cm.
Embodiment 2:
(1) graphene oxide being configured to concentration is 16mg/mL graphene oxide water solution, adds oxidation stone in the solution
The auxiliary agent of the 0.5% of ink alkene quality, described auxiliary agent is hydrochloric acid；After dispersion, it is poured on Die and mould plate relative air humidity 70% time
Naturally graphene oxide membrane is dried into；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is 30wt%, and reduction temperature is 80 DEG C, and the recovery time is 6h.
(3) graphene film after reduction is placed in 10min in the ethanol of 40 DEG C, to wash away Surface Hydrogen iodic acid, the most naturally dries in the air
Dry, obtain Graphene elastic film.
This high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and horizontal direction elastic failure percentage elongation is
36%, compression ratios is 94%, and conductivity is 800S/cm.
Fig. 1 illustrates its surface folding structure, provides the foundation (Fig. 2) for its tensile property；Fig. 3 illustrates vertical spring
Structure, provides the foundation (Fig. 4) for its elastomeric property.In conjunction with Fig. 2 and 4, it can be seen that described elastic film is by two layer graphenes
Film crosslinking forms, and described graphene membrane surface has hemispherical protuberances structure, the hemispherical protuberances knot on same layer graphene film
Structure is interconnected；The ball wall of described hemispherical protuberances structure has fold.By test, the radius 0.1 of hemispherical protuberances structure
～2mm, on ball wall, the surface density (length of fold lines in unit are) of fold is 500～2000um/um2
Embodiment 3:
(1) graphene oxide being configured to concentration is 20mg/mL graphene oxide water solution, adds oxidation stone in the solution
The auxiliary agent of the 1% of ink alkene quality, after described auxiliary agent is acetic acid dispersion, is poured on Die and mould plate at 60% time nature of relative air humidity
Dry into graphene oxide membrane；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is 35wt%, and reduction temperature is 90 DEG C, and the recovery time is 8h.
(3) graphene film after reduction is placed in 5min in the ethanol of 90 DEG C, to wash away Surface Hydrogen iodic acid, the most naturally dries in the air
Dry, obtain Graphene elastic film.
This high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and horizontal direction elastic failure percentage elongation is
50%, compression ratios is 90%, and conductivity is 1000S/cm.
Embodiment 4:
(1) graphene oxide being configured to concentration is 30mg/mL graphene oxide water solution, adds oxidation stone in the solution
The auxiliary agent of the 9% of ink alkene quality, described auxiliary agent is ammonium carbonate；After dispersion, it is poured on Die and mould plate relative air humidity 80% time
Naturally graphene oxide membrane is dried into；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is 30, and reduction temperature is 100 degrees Celsius, and the recovery time is 8h.
(3) graphene film after reduction is placed in 10min in the ethanol of 90 DEG C, to wash away Surface Hydrogen iodic acid, the most naturally dries in the air
Dry, obtain Graphene elastic film.
This high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and horizontal direction elastic failure percentage elongation is
50%, compression ratios is 90%, and conductivity is 1000S/cm.
Embodiment 5:
(1) graphene oxide being configured to concentration is 30mg/mL graphene oxide water solution, adds oxidation stone in the solution
The auxiliary agent of the 10% of ink alkene quality, described auxiliary agent is ammonium hydrogen carbonate；After dispersion, it is poured on Die and mould plate at relative air humidity 70%
Lower naturally dry into graphene oxide membrane；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is 30wt%, and reduction temperature is 70 degrees Celsius, and the recovery time is 4h.
(3) graphene film after reduction is placed in 8min in the ethanol of 80 DEG C, to wash away Surface Hydrogen iodic acid, the most naturally dries in the air
Dry, obtain Graphene elastic film.
This high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and horizontal direction elastic failure percentage elongation is
30%, compression ratios is 90%, and conductivity is 800S/cm, can be used as high-elastic conductive devices.
Embodiment 6:
(1) graphene oxide being configured to concentration is 19mg/mL graphene oxide water solution, adds oxidation stone in the solution
The auxiliary agent of the 10% of ink alkene quality, described auxiliary agent is ammonia；After dispersion, it is poured on Die and mould plate under 70% relative air humidity certainly
So dry into graphene oxide membrane；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is 20wt%, and reduction temperature is 80 degrees Celsius, and the recovery time is 8h.
(3) graphene film after reduction is placed in 10min in the ethanol of 50 DEG C, to wash away Surface Hydrogen iodic acid, the most naturally dries in the air
Dry, obtain Graphene elastic film.
This high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and horizontal direction elastic failure percentage elongation is
35%, compression ratios is 83%, and conductivity is 900S/cm.
Embodiment 7:
(1) graphene oxide being configured to concentration is 6mg/mL graphene oxide water solution, adds oxidation stone in the solution
The auxiliary agent of the 5% of ink alkene quality, described auxiliary agent is the mixture (mass ratio 1:3) of hydrochloric acid and acetic acid；After dispersion, it is poured on Die and mould plate
On under 60% relative air humidity, naturally dry into graphene oxide membrane；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is 25wt%, and reduction temperature is 70 degrees Celsius, and the recovery time is 4h.
(3) graphene film after reduction is placed in 7min in the ethanol of 80 DEG C, to wash away Surface Hydrogen iodic acid, the most naturally dries in the air
Dry, obtain Graphene elastic film.
This high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and horizontal direction elastic failure percentage elongation is
50%, compression ratios is 90%, and conductivity is 607S/cm.
Embodiment 8:
(1) graphene oxide being configured to concentration is 23mg/mL graphene oxide water solution, adds oxidation stone in the solution
The auxiliary agent of the 7% of ink alkene quality, described auxiliary agent is the mixture (mass ratio 2:1) of ammonium hydrogen carbonate and ammonium carbonate；After ultrasonic disperse,
It is poured on Die and mould plate under 50% relative air humidity, naturally dries into graphene oxide membrane；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is 26wt%, and reduction temperature is 70 degrees Celsius, and the recovery time is 8h.
(3) graphene film after reduction is placed in 10min in the ethanol of 60 DEG C, to wash away Surface Hydrogen iodic acid, the most naturally dries in the air
Dry, obtain Graphene elastic film.
This high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and horizontal direction elastic failure percentage elongation is
30%, compression ratios is 90%, and conductivity is 1000S/cm, can be used as high-elastic conductive devices.
Embodiment 9:
(1) graphene oxide being configured to concentration is 30mg/mL graphene oxide water solution, adds oxidation stone in the solution
The auxiliary agent of the 8% of ink alkene quality, described auxiliary agent is the mixture (mass ratio 1:1) of ammonium chloride and ammonium hydrogen carbonate；After dispersion, it is poured on
Under 80% relative air humidity, graphene oxide membrane is naturally dried on Die and mould plate；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is 35wt%, and reduction temperature is 100 degrees Celsius, and the recovery time is 4h.
(3) graphene film after reduction is placed in 5min in the ethanol of 90 DEG C, to wash away Surface Hydrogen iodic acid, the most naturally dries in the air
Dry, obtain Graphene elastic film.
This high flexibility Graphene heat conducting film is resistant to repeatedly bend more than 100,000 times, and horizontal direction elastic failure percentage elongation is
50%, compression ratios is 90%, and conductivity is 1000S/cm.
Embodiment 10:
(1) graphene oxide of 100 weight portions being configured to concentration is 6mg/mL graphene oxide water solution, in the solution
Add the ammonium chloride of 0.1 weight portion, after ultrasonic disperse, be poured on Die and mould plate, natural under relative air humidity (as shown in table 1)
Dry into graphene oxide membrane；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is 30wt%, and reduction temperature is 80 degrees Celsius, and the recovery time is 4h.
(3) graphene film after reduction is placed in 5min in the ethanol of 40 DEG C, to wash away hydroiodic acid, the most naturally dries,
To Graphene elastic film A1～A10.
Table 1: the performance of the product obtained under different relative humiditys
As can be seen from the above table, under low relative humidity (50%), graphene film is not enough to form the poroid knot of continuous print
Structure does not the most stretch and the elasticity of compression；Along with the raising of relative humidity, its cavernous structure molding, and also aperture is increasingly
Greatly, fold surface density is more and more higher, and therefore its Compression and Expansion performance steps up；After relative humidity is more than 80%, its property
Can be basically unchanged, can be attributed to, the regulation and control of its structure are reached capacity by relative humidity.
Embodiment 11:
(1) graphene oxide of 100 weight portions being configured to concentration is 6mg/mL graphene oxide water solution, in the solution
Add the ammonium chloride of 0.1 weight portion；After ultrasonic disperse, it is poured on Die and mould plate, naturally dries into for 80% time at relative air humidity
Graphene oxide membrane；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.Described hydroiodic acid solution
HI content is as shown in table 2, and reduction temperature is 80 degrees Celsius, and the recovery time is 4h.
(3) graphene film after reduction is placed in 5min in the ethanol of 40 DEG C, to wash away hydroiodic acid, the most naturally dries,
To Graphene elastic film B1～B10.
Table 2: the performance of the product of different hydro iodic acid solution HI content (wt%)
As can be seen from the above table, under low-concentration hydrogen iodic acid (15%), graphene oxide membrane reduction dynamics is inadequate, is not enough to
Make graphene film form continuous print cavernous structure, the most do not stretch and the elasticity of compression；Along with carrying of hydriodic acid concentration
Height, its cavernous structure molding, and also aperture is increasing, and fold surface density is more and more higher, and therefore its Compression and Expansion performance is progressively
Improve；After hydriodic acid concentration is more than 37%, its performance has declined, and can be attributed to too high hydriodic acid concentration and make
Surface reduction transitional effects hydroiodic acid enters inside graphene oxide membrane so that membrane material is uneven, and then damage performance.
Claims (6)
1. a Graphene elastic film, it is characterised in that described elastic film is formed by the crosslinking of two-layer graphene film, described stone
Ink alkene film surface has hemispherical protuberances structure, and the hemispherical protuberances structure on same layer graphene film is interconnected；Described half
The ball wall of ball bumps structure has fold.
Graphene elastic film the most according to claim 1, it is characterised in that the radius of described hemispherical protuberances structure
0.1～2mm, on ball wall, the surface density (length of fold lines in unit are) of fold is 500～2000um/um2。
3. the preparation method of a Graphene elastic film, it is characterised in that comprise the steps of:
(1) graphene oxide of 100 weight portions being configured to concentration is 6～30mg/mL graphene oxide water solution, in the solution
Adding the auxiliary agent of 0.1-10 weight portion, described auxiliary agent is the volatilizable and degradable little molecule of low temperature；After ultrasonic disperse, it is poured on
On Die and mould plate, under certain relative air humidity, naturally dry into graphene oxide membrane；
(2) the oxidation elastic graphite alkene thin film after drying reduces in hydriodic acid aqueous solution.
(3) graphene film after reduction is placed in the ethanol of 40-90 DEG C 5～10min, to wash away Surface Hydrogen iodic acid, then natural
Dry, obtain Graphene elastic film.
Method the most according to claim 3, it is characterised in that the relative air humidity in described step 1 is 50-80%.
5. method as claimed in claim 3, it is characterised in that described auxiliary agent selected from ammonium hydrogen carbonate, ammonium chloride, ammonium carbonate,
One or more in hydrochloric acid, acetic acid and ammonia.
6. method as claimed in claim 3, it is characterised in that described hydroiodic acid Solution H I content is 15 35wt%, also
Former temperature is 70 100 degrees Celsius, and the recovery time is 4-8h.
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| CN107863905A (en) * | 2017-10-16 | 2018-03-30 | 北京理工大学 | A kind of electric energy generating method based on graphene oxide membrane |
| CN108724867A (en) * | 2018-06-06 | 2018-11-02 | 合肥工业大学 | A kind of porous graphene driver of double stimulus response, preparation method and application |
| CN108899216A (en) * | 2018-07-09 | 2018-11-27 | 杭州高烯科技有限公司 | A kind of high density azepine graphene film and preparation method thereof |
| CN111807355A (en) * | 2020-08-10 | 2020-10-23 | 北京航空航天大学 | Preparation method of in-plane isotropic high-orientation densified graphene film |
| WO2023125351A1 (en) * | 2021-12-27 | 2023-07-06 | 华为技术有限公司 | Carbon material and use thereof |
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